Summary report for Directory: home/diska/04src0422

Report generated May 27, 2004; 15:50:19

Unit cell

8423 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack c2

a (Angstrom) 23.4352 +/- 0.0010

b (Angstrom) 18.0929 +/- 0.0009

c (Angstrom) 20.9394 +/- 0.0009

alpha (°) 90.000

beta (°) 118.729 +/- 0.002

gamma (°) 90.000

Volume (A**3) 7785.6 +/- 0.6
Mosaicity (°) 1.193 +/- 0.002

Symmetry used in scalepack	c2
a (Angstrom)	23.4352 +/- 0.0010
b (Angstrom)	18.0929 +/- 0.0009
c (Angstrom)	20.9394 +/- 0.0009
alpha (°)	90.000
beta (°)	118.729 +/- 0.002
gamma (°)	90.000
Volume (A**3)	7785.6 +/- 0.6
Mosaicity (°)	1.193 +/- 0.002

Data collection

Summary

Total number of images collected	191
Total exposure time	62.8 minutes
Data collection exposure time	61.7 minutes
Data collection wall-clock time	76.2 minutes

Experimental Conditions

Wavelength	0.71073 A
Cryostat setting	120.00K
Crystal to detector distance	40.00 mm

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Used in scaling
data collection	s01f	141	`282.0`° phi	2.000°	20 seconds	Yes
data collection	s02f	42	`84.0`° omega	2.000°	20 seconds	Yes
Phi/Chi	i01f - i08f	8			8 seconds

Scalepack Scaling

Deleted observations

Rejected	`299`
Overload or incomplete profile	`1522`
Sigma cutoff	`97`
High resolution limit	`87`

Final Data Set

Scale factor range	7.65-10.00
Number of 'full' reflections	`9139`
Number of 'partial' reflections	`27099`
Total number of integrated reflections	`33199`
Total number of unique reflections	`8995`
Data completeness	`97.2%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`79.7`
Average Sigma(I)	`4.2`
Overall R-merge (linear)	`0.066`

Sadabs Results

Parameter refinement on 21187 reflections reduced R(int) from 0.1714 to 0.0514

Before rejection, 34431 reflections total and 9237 unique

After rejection, 33556 reflections total and 9227 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   15.6  0.0605   0.815 - 1.166   0.928 - 1.315   1.458   25783   16986
    2  -15.0  0.0763   0.631 - 0.796   0.978 - 1.316   1.517    7773    4912

Ratio of minimum to maximum apparent transmission: 0.705540

Metadata

Group Service

Operator Peter Horton

Sample Owner Dr Craig Matthews

Local Code LJD394Zn

Formula C87 H75 N39 O24 Cl6 Zn3

Crystal Colour Light Green

Crystal Habit Slab

Crystal Size 0.22 x 0.2 x 0.07 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Peter Horton
Sample Owner	Dr Craig Matthews
Local Code	LJD394Zn
Formula	C87 H75 N39 O24 Cl6 Zn3
Crystal Colour	Light Green
Crystal Habit	Slab
Crystal Size	0.22 x 0.2 x 0.07 (mm3)
Temperature	120(K)
Generator	50 (kV) 85 (mA)
Primary Solvent
Other Solvents

File Explanations

SampleCode.zip
      SampleCode.hkl - data corrected using SADABS
      SampleCode_merge_none.hkl - equivalents and friedels kept separate (See "Final Data Set" table in this report)
      SampleCode.p4p - skeleton p4p file for use with XPREP
      SampleCode.htm - this summary file

Southampton CIF entry fields

_exptl_absorpt_process_details   'SADABS V2.10 (Sheldrick, G.M., 2003)'

_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength   0.71073
_diffrn_radiation_type                MoK\a
_diffrn_radiation_source            'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    '10cm confocal mirrors'
_diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method          '\f & \w scans'
_diffrn_detector_area_resol_mean   9.091

_computing_data_collection
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'

Software References

Unit Cell Determination using DirAx:
Duisenberg AJM. Indexing in Single-Crystal Diffractometry with an Obstinate List of Reflections. Journal of Applied Crystallography 1992; 25: 92-96.
Duisenberg AJM, Hooft RWW, Schreurs AMM, Kroon J. Accurate cells from area-detector images. Journal of Applied Crystallography 2000; 33: 893-898.

Diffractometer control and strategy calculation using COLLECT:
Hooft RWW. COLLECT data collection software, Nonius B.V., 1998.

Standard Data Reduction using HKL(Denzo & Scalepack):
Otwinowski Z, Minor W. Processing of X-ray diffraction data collected in oscillation mode. Macromolecular Crystallography, Pt A. 1997; 276: 307-326.

Absorption Correction
Sheldrick, G. M. SADABS - Bruker Nonius area detector scaling and absorption correction - V2.10

Non-Standard Data Reduction using EvalCCD:
Duisenberg AJM, Kroon-Batenburg LMJ, Schreurs AMM. An intensity evaluation method: EVAL-14. Journal of Applied Crystallography 2003; 36: 220-229.

For more information visit the service web site at: http://www.soton.ac.uk/~xservice/